反应 #51274

ord-fb17e6201ae24177862d7baad47c5a19

溶剂

反应条件

温度
7.5°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The solution obtained
  2. 2
    workup.STIRRINGthe reaction mixture is stirred for one hour at room temperature
  3. 3
    萃取extracted with ethyl ether
  4. 4
    其他the organic phase is separated
  5. 5
    干燥dried over magnesium sulphate
  6. 6
    其他evaporated
  7. 7
    其他46.00 g (130%) of the expected compound are collected in the form of an orange oil

实验过程

40.00 g (140.2 mmol) of 2,4-di-tert-butyl-6-bromophenol and 400 ml of DMF are introduced into a one liter three-necked flask. The solution obtained is cooled to 5-10° C., 4.70 g of sodium hydride are added and the mixture is stirred at 10° C. for 30 minutes. 11.7 ml (154.0 mmol) of chloromethyl methyl ether are then added dropwise and the reaction mixture is stirred for one hour at room temperature. The reaction mixture is poured into a 1N HCl/ethyl ether mixture and extracted with ethyl ether and the organic phase is separated by settling, dried over magnesium sulphate and evaporated. 46.00 g (130%) of the expected compound are collected in the form of an orange oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06849658B2uspto-grants-2005_02